反応 #1750900

反応方程式

Hydrochloric acid

methyl 3-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)benzoate

sodium hydroxide

→

title compound

収率 69.3%

3-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)benzoic acid

収率 69.3%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   抽出the aqueous layer was extracted three times with ethyl acetate/tetrahydrofuran
2. 2
   洗浄Combined organic layer was washed with saturated brine
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   ろ過filtrated
5. 5
   その他The solvent was evaporated under reduced pressure
6. 6
   ろ過the residue was filtrated
7. 7
   洗浄washed with ethyl acetate/hexane

実験手順

To a solution of methyl 3-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)benzoate (225 mg, 0.64 mmol) in tetrahydrofuran (5.0 mL) was added 1N sodium hydroxide (2.5 mL), and the mixture was stirred at room temperature for 24 hr. 1N Hydrochloric acid was added to the mixture (pH=3), and the aqueous layer was extracted three times with ethyl acetate/tetrahydrofuran. Combined organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and filtrated. The solvent was evaporated under reduced pressure, and the residue was filtrated, and washed with ethyl acetate/hexane to give the title compound (150 mg, 69%) as a white powder.

出典